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Cesium carbonate → 5-chloro-N-(5-fluoro-6-((4S,6S)-4-methyl-2-(4-nitrobenzamido)-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-4-yl)pyridin-2-yl)picolinamide

HRID 930311
ノート
印刷プレビュー

反応式

HRID 930311 の反応式
Br[C:2]1[N:7]=[C:6]([C@:8]2([CH3:30])[CH2:13][C@@H:12]([C:14]([F:17])([F:16])[F:15])[O:11][C:10]([NH:18][C:19](=[O:29])[C:20]3[CH:25]=[CH:24][C:23]([N+:26]([O-:28])=[O:27])=[CH:22][CH:21]=3)=[N:9]2)[C:5]([F:31])=[CH:4][CH:3]=1.[Cl:32][C:33]1[CH:34]=[CH:35][C:36]([C:39]([NH2:41])=[O:40])=[N:37][CH:38]=1.C(=O)([O-])[O-].[Cs+].[Cs+].CC1(C)C2C=CC=C(P(C3C=CC=CC=3)C3C=CC=CC=3)C=2OC2C1=CC=CC=2P(C1C=CC=CC=1)C1C=CC=CC=1>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].O1CCOCC1>[Cl:32][C:33]1[CH:34]=[CH:35][C:36]([C:39]([NH:41][C:2]2[CH:3]=[CH:4][C:5]([F:31])=[C:6]([C@:8]3([CH3:30])[CH2:13][C@@H:12]([C:14]([F:17])([F:16])[F:15])[O:11][C:10]([NH:18][C:19](=[O:29])[C:20]4[CH:25]=[CH:24][C:23]([N+:26]([O-:28])=[O:27])=[CH:22][CH:21]=4)=[N:9]3)[N:7]=2)=[O:40])=[N:37][CH:38]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10796Cesium carbonateHCID 6360441,1'-(9,9-Dimethyl-9H-xanthene-4,5-diyl)bis(1,1-diphenylphosphine)HCID 218831585-Chloropyridine-2-carboxamide2 回HCID 86732139N-((4S,6S)-4-(6-bromo-3-fluoropyridin-2-yl)-4-methyl-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-2-yl)-4-nitrobenzamide

生成物 1

HCID 86732138
5-chloro-N-(5-fluoro-6-((4S,6S)-4-methyl-2-(4-nitrobenzamido)-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-4-yl)pyridin-2-yl)picolinamide

試薬・触媒・溶媒 2

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 312751,4-Dioxane溶媒

反応条件

温度
110 °C

実験手順

A mixture of A sealable vial was charged with N-((4S,6S)-4-(6-bromo-3-fluoropyridin-2-yl)-4-methyl-6-(trifluoromethyl)-5,6-dihydro-4H-1,3-oxazin-2-yl)-4-nitrobenzamide (8a, 0.297 g, 0.588 mmol), 5-chloropicolinamide (intermediate 18, 0.101 g, 0.647 mmol), cesium carbonate (0.479 g, 1.470 mmol, Aldrich), Pd2(dba)3 (0.040 g, 0.044 mmol, Strem), (9,9-dimethyl-9H-xanthene-4,5-diyl)bis(diphenylphosphine) (0.102 g, 0.176 mmol, Aldrich), and 1,4-dioxane (4 mL). The reaction was purged with Argon and heated to 110° C. overnight. The reaction mixture was filtered through celite and the filter cake was washed with EtOAc. The filtrate was washed with water and brine, dried over sodium sulfate and concentrated under reduced pressure. The crude material was purified via silica gel flash chromatography (gradient 0-35% EtOAc in hexanes) to afford the title compound as a light yellow solid. MS m/z=581 [M+H]+. Calculated for C24H17ClF4N6O5: 580.

後処理

  1. additionA mixture of A sealable vial
  2. customThe reaction was purged with Argon
  3. filtrationThe reaction mixture was filtered through celite
  4. washthe filter cake was washed with EtOAc
  5. washThe filtrate was washed with water and brine
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe crude material was purified via silica gel flash chromatography (gradient 0-35% EtOAc in hexanes)

出典と根拠

ORDレコード
ord-30126cafbf714a03b5d19193fec02a04
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09296734B2

反応ノート

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